Phthalic Anhydride → HCID 131718923, 화합물

HRID 1608914

반응식

HRID 1608914 반응식
[NH2:1][C:2]1C=[C:4]2[C:9](=[CH:10][CH:11]=1)C(S(O)(=O)=O)=CC=C2.[C:16]1(=[O:26])[O:21][C:19](=O)[C:18]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:17]12.[Na+].[NH2:28][C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[C:35]([S:39]([O-:42])(=[O:41])=[O:40])=[CH:34][CH:33]=[CH:32]2.C([NH+](CC)CC)C>N1C=CC=CC=1>[NH+:1]1[CH:2]=[CH:11][CH:10]=[CH:9][CH:4]=1.[C:19]1(=[O:21])[N:28]([C:29]2[CH:30]=[C:31]3[C:36](=[CH:37][CH:38]=2)[C:35]([S:39]([O-:42])(=[O:40])=[O:41])=[CH:34][CH:33]=[CH:32]3)[C:16](=[O:26])[C:17]2=[CH:25][CH:24]=[CH:23][CH:22]=[C:18]12

참가 물질

6

반응물 4

HCID 6811Phthalic AnhydrideHCID 664706-Aminonaphthalene-1-sulphonic acidHCID 1385867TriethylammoniumHCID 23696805Sodium 6-aminonaphthalene-1-sulphonate

생성물 1

HCID 131718923HCID 131718923, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

223 g (1 mol) of 6-amino-1-naphthalenesulfonic acid and 148 g (1 mol) of phthalic anhydride are boiled for 0.5 h in 1 liter of pyridine. After boiling, the reaction mixture is left at room temperature for 16 h. The precipitated product is filtered and washed with pyridine and water, and then recrystallized from boiling water. Yield 298 g (69%); mp 234°-237° C.; Anal. Calcd. for C23H16N2SO5 :C 63.88, H 3.73, N 6.48, S 7.42; Found:C 63.74, H 3.81, N 6.52, S 6.99. When the 6-phthalimido-1-naphthalenesulfonic acid pyridinium salt was synthesized starting from 6-amino-1-naphthalenesulfonic acid sodium salt or triethylammonium salt, the calculated yields were 63% and 58% respectively.

후처리

  1. filtrationThe precipitated product is filtered
  2. washwashed with pyridine and water
  3. customrecrystallized
  4. customthe calculated yields

출처 및 근거

ORD 기록
ord-05251847db624057a3846b096fcc6b76
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399487

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